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CPE-TiO2

Electrochemical detection of Pb metal ion

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CPE-TiO2

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  1. Hasil Penelitian CARBON PASTE ELECTRODE/Ti02 (CPE-TiO2) MODIFIED OF HEKSA(p-tert-BUTYL)HEKSA(ETYLESTER)CALIX[6] ARENE (BEK6) IONOPHORE AS Pb2+ DETECTION SENSOR IRWAN F1C1 13 072 Supervisor II Dr. H. Nasriadi Dali, M.Si Supervisor I Prof. Dr. H. Muh.Nurdin, M.Sc

  2. INTRODUCTION Industry leading of waste Enviromental pollution Based on the regulation of goverment Republic of Indonesia No. 82 (2001) that the contain of Pb in water no more 0.03 ppm (Rahman, 2006). Industry waste Toxic impact of Pb on human

  3. INTRODUCTION Determination methods of Pb 1 High Sensitivity 2 Low Limite detection AAS The dissaventages: 1. The Analysis according to atomization of substance on solution is less spesific for ion. 2. High cost (Sulfani, 2014) 3 Voltammetry Low cost 4 Fast Time Analysis 5 Convenientuse and sample preparation Electrochemistry ICP-MS (Putra dan Pirim, 2015)

  4. INTRODUCTION Voltammetry 1. Graphite 2. Paraffin Modified • Surface area is large • Good thermal stability • Providing a more active on the electrode surface • (Ensafiet al., 2013). Potensiostat RE CE WE Electrodeusing of Hg Carbon Paste Electrode (CPE) Toxicity (Suliana, 2014) BEK6

  5. STATE OF THE ART 2017 CARBON PASTE ELECTRODE/Ti02 (CPE-TiO2) MODIFIED OF HEKSA(p-tert-BUTIL) HEKSA(ETILESTER)CALIX [6]ARENE (BEK6) IONOPHORE AS Pb2+ DETECTION SENSOR 2017 2015 2014 2012

  6. PROBLEM STATEMENTS 1 • How are the effect of adding BEK6 ionophore as modifier to the • performance CPE/TiO2? 2 • How are the performance CPE/TiO2 modified BEK6 ionophore • in determinan ion Pb2+?

  7. PURPOSE 1 • To knowing the effect of adding BEK6 ionophore as modifier to the performance of CPE/TiO2. 2 • To knowing the performance of CPE/TiO2 modified BEK6 • ionophore to determination of Pb2+.

  8. BENEFITS 1 2 • To provide an information about • the effect of adding BEK6 ionophore as modifier to the • performance of CPE/TiO2. • To provide an information about the • Performance of CPE/TiO2 modified • BEK6 ionophore to determination of • Pb2+.

  9. RESEARCH METHODS Synthesis TiO2 Ionophore XRD TiO2 Anatase BEK6 CPE/TiO2 CPE/TiO2-BEK6 FTIR Characterization SEM Performance test in K3 [Fe(CN6)] Parameter test CPE/TiO2-BEK6 in determination of Pb2+

  10. RESEARCH METHODS 1. Preparation of TiO2 Anatase (Thamapat et al., 2008) Characterization of XRD nanopartikel TiO2 anatase

  11. RESEARCH RESULT 2. Characterized by FTIR A. CPE/TiO2 material B. CPE/TiO2-BEK6material A CPE/TiO2-BEK6material B

  12. RESEARCH RESULT 3. Characterized by SEM A B 1 µm 10 µm D C 10 µm 1 µm CPE/TiO2 material :(A) magnifation 1000 x (B) magnifation 10.000 x and CPE/TiO2-BEK6 material­: (C) magnifation 1000 x(D) magnifation 10.000 x

  13. RESEARCH RESULT 4. Performance test of, CPE/TiO2andCPE/TiO2-BEK6 EPK/TiO2 EPK/TiO2-BEK6 0,005 g Fe(CN)63-(aq) + e- ⇌ Fe(CN)64-(aq) Voltamogram EPK/TiO2and EPK/TiO2-BEK6 in K3[Fe(CN)6]

  14. RESEARCH RESULT 5. Effect of modifier mass variations of the BEK6 to CPE/TiO2 performance in Pb2+ solutions BEK60,005 g BEK6 0,010 g BEK6 0,015 g Voltamogram EPK/TiO2-BEK6 with variations of modifier mass

  15. RESEARCH RESULT 6. Effect of supporting electrolyte pH to CPE/TiO2 - BEK6 performance in Pb2+ solutions pH 3 pH 4 pH 5 pH 6 Usulan mekanisme pembentukan kompleks BEK6 dengan Pb2+ Plot between the pH of the solution and the peak current of the results measurenment Voltamogram EPK/TiO2-BEK6 to influence variations of pH citratebuffer in the measurenment of Pb2+

  16. RESEARCH RESULT 7. Effect of scan ratevariation to CPE /TiO2 - BEK6 performance in Pb2+ solutions Scanrate 0,1 v/s Scan rate 0,3 v/s Scanrate 0,5 v/s Scanrate 0,8 v/s A B Voltamogramoptimum scan rate test plot between of scan rateand the current of the results measurenment

  17. RESEARCH RESULT 8. Determination of linearity and detection limit (LD) Table data linearity and limit detection

  18. RESEARCH RESULT 9. Determinan of measurenmentrepeability Histogram repeability test of Pb2+ measurement in DPV

  19. RESEARCH RESULT 10. Selectivity Pb2+ dan Ni2+ 1 ppm Pb2+ 1 ppm Cyclic Voltamogram selectivity tes of Pb2+ measurement

  20. CONCLUSION 1 The optimum modifier composition of electrode with BEK6 ionofor composition of 0.005 g is indicated by anodic peak current (Ipa) of 8.64x 10-5A and cathodic peak current (Ipc) -8,72x 10-5A. Other factors Which affects the pH of the solution and the scan time rate. The optimum measurement condition of EPK / TiO2-BEK6 in detecting Pb2+ions is at pH 5 with scan speed of 0.8V / s 2 The detection limit obtained from the measurement of EPK/TiO2-BEK6 on Pb2+ions is 0.0257 ppm and the repeatability of EPK/TiO2-BEK6 performance is 0.83%. The low% RSD value states the precision level of EPK/TiO2-BEK6 quite well

  21. 99 124 7 19 Th A N K Adamantium Thorium Nitrogen Potassium 8 92 39 O U Y Uranium Yitrium Oxygen

  22. RESEARCH METHODS 1. Preparation of TiO2 Anatase and Rutile a. Preparation of TiO2Anatase b. Preparation of TiO2Rutile TiO2degussa powder TiO2degussa powder 10 grams 10 grams Calcinateed for 3 hours at 800 ᵒC Calcinated for 3 hours at 300 ᵒC TiO2Rutile TiO2Anatase

  23. RESEARCH METHODS 2. Preparations of CPE, CPE/TiO2andCPE/TiO2-BEK6 a. Preparation of CPE Graphite Paraffin oil • Ratio of graphite:paraffin is 5:5 • Paraffin heated at 80 oC Copper wire Agency electrode • Polished electrode surface till • smooth, flat and shiny. Carbon paste

  24. RESEARCH METHODS b. Preparation of CPE/TiO2 Graphite Paraffin oil • Ratio of graphite:paraffin:TiO2 are 3:2:5, 3:3:4, 3:4:3 and 3:5:2 • Paraffin heated at 80 oC Copper wire TiO2 Powder Agency electrode • Polished electrode surface • till smooth, flat and shiny. Carbon paste Anatase Rutile

  25. RESEARCH METHODS c. Preparation of CPE/TiO2-BEK6 • Good ratio of graphite:paraffin:TiO2 • added BEK6 with weight variations • are 0,001; 0,010 and 0,015 g • Paraffin heated at 80 oC Graphite Paraffin oil Copper wire TiO2 Powder BEK6 Agency electrode • Polished electrode surface • till smooth, flat and shiny. Carbon paste

  26. RESEARCH METHOD 3. Performance test of CPE, CPE/TiO2andCPE/TiO2-BEK6 in K3[Fe(CN)6] Potensiostat • Measurenments of range potential from -1V to • 1V with scan rate of 0.1 V / s 1 2 3 1. Ag/AgCl 2. Platinum wire 3. CPE, CPE/TiO2, CPE/TiO2-BEK6 K3[Fe(CN)6] 0,01 M Voltammogram

  27. RESEARCH METHODS 4. Effect of modifier mass variations of the BEK6 to CPE/TiO2 performance in Pb2+ solutions • Measurenments of range potential from -1V to • 1V with scan rate of 0.1 V / s Potensiostat 1 2 3 1 Ag/AgCl • Voltammogram 2 Platinum wire 3 CPE/TiO2-BEK6 with weight of BEK6 are 0,001; 0,010 and 0,015 g • Compared to obtain • composition the good • electrode Voltammetry cell 4 Voltammetry cell (10 mL Pb2+ 1 ppm, 10 mL NaCl 0,1 M and 5 mLphospate buffer pH 8)

  28. RESEARCH METHODS 5. Effect of supporting electrolyte pH to CPE/TiO2 - BEK6 performance in Pb2+ solutions • Measurenments of range potential from -1V to • 1V with scan rate of 0.1 V / s Potensiostat 1 2 3 1 Ag/AgCl 2 • Voltammogram Platinum wire 3 CPE/TiO2-BEK6 with best composition 4 Voltammetry cell (10 mL Pb2+ 1 ppm, 10 mL NaCl 0,1 M and 5 mLphospate buffer pH 8) 4 • Compared to obtain of • optimum pH condition Variations buffer phospatepH 5,6, 7 and 8)

  29. RESEARCH METHOD 6. Effect of scan ratevariation to CPE /TiO2 - BEK6 performance in Pb2+ solutions • Measurenments of range potential from-1V to • 1V with variation scan rate are 0.01; 0.02; 0.04; • 0.05; 0.06; and 0.08 V/s. Potensiostat 1 2 3 1 Ag/AgCl • Voltamogram 2 Platinum wire 3 CPE/TiO2-BEK6 best composition 4 Solutions • Compared to obtain • of good scan rate 4 Voltammetry cell (10 mL Pb2+ 1 ppm, 10 mL NaCl 0,1 M and 5 mLphospate buffer pH 8)

  30. RESEARCH METHOD 7. Determination of linearity and detection limit (LD) • Measured using Differential Pulse Voltammety (DPV) and Square Wave Voltametri • (SWV) methods Potensiostat 1 2 3 1 Ag/AgCl • Voltammogram 2 Platinum wire 3 CPE/TiO2-BEK6 best composition • Determination the linear • range of the calibration curve Solutions 4 4 Voltammetry cell (10 mL Pb2+ 1 ppm, 10 mL NaCl 0,1 M and 5 mLphospate buffer pH 8)

  31. RESEARCH METHOD 8. Determinan of measurenmentrepeability and dan % recovery • Measured using Differential Pulse Voltammety (DPV) and Square Wave Voltametri • (SWV) methods Potensiostat 1 2 3 1 Ag/AgCl • Voltammogram 2 Platinum wire 3 6 electrodes CPE/TiO2-BEK6 best composition Solutions 4 • Determination the • repeability and % recovery 4 Voltammetry cell (10 mL Pb2+ 1 ppm, 10 mL NaCl 0.1 M and 5 mLphospate buffer pH 8)

  32. RESEARCH METHOD 9. Characterization CPE CPE/TiO2 Good composition CPE/TiO2-BEK6 FTIR SEM

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